通过硅胶、大孔树脂、葡聚糖凝胶Sephadex LH-20和HPLC等多种色谱分离方法相结合,从长梗喉毛花Comas-toma pedunculatum(Royle ex D.Dou)Holub全草乙醇提取物的正丁醇萃取部位中分离得到13个化合物,其中9个皂苷类,4个黄酮碳苷类;根据化合物的理化性质和波谱数据鉴定化合物的结构为柴胡皂苷元F(1),3-O-β-D-呋糖基柴胡皂苷元F(2),风轮菜苷ⅩⅤ(3),柴胡皂苷A(4),6″-乙酰基柴胡皂苷A(5),风轮菜苷Ⅰ(6),柴胡苷Ⅰ(7),风轮菜苷Ⅻ(8),柴胡皂苷b3(9),异牡荆苷(10),当药黄素(11),异荭草素(12),3',4',5-三羟基-7-甲氧基-6-C-β-D-吡喃葡萄糖黄酮苷(13)。化合物1～10,12,13均为首次从该属植物中分离得到。
To develop a simple and rapid purification method of rohitukine from the stem bark of Dysoxylum binectariferum. A L9 （34） orthogonal test was designed to optimize the extraction condition. Rohitukine in the plant extract was purified by using solvent-solvent partition and cation exchange resion （CER）. Five different types of packing materials, including XAD-2 resin, polyamide, Sephadex LH-20, ODS and CER, were compared and CER showed the best capacity for rohitukine separation. The purification procedure was optimized as follows： the plant material powder was extracted with 70% ethanol （v/m = 60） by ultrasonic agitation for 60 min, then the 70% ethanol extract was dissolved in aqueous solution （pH 1, adjusted with 0.5 mol/L HCl） and extracted with equal volume of n-butanol. The aqueous layer was retained and the pH was adjusted to 10 with 25% aqueous ammonia and a solventsolvent partition was performed with equal volume of n-butanol. The obtained n-butanol extract was dissolved in aqueous solution （pH 1, adjusted with 0.5 mol/L HCl）, and purified by a CER column eluting with H2O and 70% ethanol （pH 10, adjusted with 25% aqueous ammonia）, successively. Rohitukine existed in 70% ethanol eluate, with a purity up to 53.3%. The method developed in this study provides a simple and rapid approach for the preparation of rohitukine from the stem bark ofD. binectariferum.
